반응 #5716

ord-3394f386594347eeac4f17cc00376730

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGwas stirred for 10 minutes
  2. 2
    workup.STIRRINGThe mixture was stirred for a further 2.5 hours
  3. 3
    추출The reaction solution was extracted in toluene with 1N sodium hydroxide solution
  4. 4
    건조The combined toluene phases were dried
  5. 5
    여과the drying agent was filtered off under suction
  6. 6
    세척washed with toluene
  7. 7
    기타Evaporation of the solvent

실험 절차

177.3 g of the δ-lactone from c) were suspended in 1250 ml of toluene while stirring. After the addition of 138.6 g of benzoic anhydride the mixture was stirred for 10 minutes. Then, 2.5 ml of perchloric acid were added. The mixture was stirred for a further 2.5 hours. The reaction solution was extracted in toluene with 1N sodium hydroxide solution and then with water. The combined toluene phases were dried, the drying agent was filtered off under suction and washed with toluene. Evaporation of the solvent gave 237.2 g (103.4%) of rac-(2RS,3RS,5SR)-3-benzoyloxy-2-hexyl-5-undecyl-δ-valerolactone, which was used in the next step without purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05245056uspto-grants-1993_09